氮杂环羧酸及类卤素配位聚合物的构筑和性质研究
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摘要
羧酸类配体配位能力强、配位方式灵活,其与金属离子配位得到的配位聚合物通常具有新颖多变的结构,在多孔材料、分子磁性材料等方面有重要研究意义。而叠氮、硫氰酸根等类卤素配体配位方式多样,能有效传递不同的磁交换作用,在分子磁性材料研究中也受到广泛关注。类卤素配体可以和羧酸类配体共同参与配位,形成混合桥联化合物,不仅丰富了配位聚合物结构化学和晶体工程研究,而且两种桥联配体对金属顺磁中心之间的磁交换有不同的传递作用,使得整个化合物在磁学性质上具有一定的新颖性。本论文选择叠氮、硫氰酸根、氮杂环羧酸或二羧酸为单一或混合桥联配体,与过渡或稀土金属离子配位合成了24个双核,一维链或二维层的配位聚合物,在结构分析基础上对部分化合物的结构组装规律和磁学性质进行了较细致的研究。本论文的研究工作主要分为以下几个部分:
1哒嗪二甲酸的配位化学及抗衡离子对晶体结构组装的影响:(1)首先,我们采用3,6-哒嗪二甲酸(H_2pzdc)配体与金属Mn(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)及Zn(Ⅱ)离子在水热条件下合成得到了一系列双核化合物。其中最值得一提的是Mn(Ⅱ)形成的结构独特的双核阴离子[Mn_2(pzdc)_3]~(2-),该化合物中三个pzdc配体围绕一个C_3对称轴与两个金属离子配位,形成三棱柱结构。而金属Co(Ⅱ)、Ni(Ⅱ)或Zn(Ⅱ)形成一种边边配位的中性平面分子[M_2(pzdc)_2(H_2O)_4]。这种结构差异的出现可以归因于这些金属离子半径的差异。(2)在Mn(Ⅱ)的化合物中,三棱柱阴离子[Mn_2(pzdc)_3]~(2-)单元有丰富的未配位羧酸氧原子,以这些氧原子为潜在的配位点或是氢键受体,可以将这种阴离子结构当做“配合物配体”用于构建新的金属-有机配位聚合网络或氢键超分子网络。考虑到这种配合物配体策略,我们在合成化合物的过程中引入了抗衡离子(NH_4~+,K~+或Na~+)从而得到了一系列金属Mn(Ⅱ)和Zn(Ⅱ)的化合物。这些化合物都包含双核三棱柱结构单元[M_2(pzdc)_3]~(2-),这种阴离子单元又可以和不同的阳离子(NH_4~+,K~+或Na~+)连接形成三维的配位或氢键网络。然而对于金属Co(Ⅱ)和Ni(Ⅱ)的体系中,不管是否引入抗衡离子,都只能得到上述的边边配位的中性分子结构。
2含甜菜碱类共配体的叠氮-羧基混桥化合物的结构与磁性:叠氮离子在与负电性羧酸根离子的配位竞争中处于劣势,因此利用通常的二羧酸配体难以得到叠氮-羧基混桥配合物。我们试图通过降低二羧酸配体的负电荷来降低二羧酸配体的竞争能力,使之与叠氮配体相匹配,从而得到含有羧酸-叠氮混桥的化合物。基于这种策略,我们采用了甜菜碱类双羧酸有机配体,以这种配体作为辅助配体,在叠氮存在下,与金属Ni(Ⅱ),Co(Ⅱ),Mn(Ⅱ)和Cu(Ⅱ)配位得到了一系列叠氮-羧基混桥化合物,其中Ni、Co、Mn的化合物是同晶结构。其中金属离子通过叠氮-羧基三重桥(一个EO叠氮桥和两个syn-syn羧基桥)和两重EO叠氮桥连接成负电性聚合链,链间又通过正电性有机基团连接成层。磁性研究表明上述三重桥在Co(Ⅱ)、Ni(Ⅱ)化合物中传递铁磁交换,而在Mn(Ⅱ)化合物中传递反铁磁交换。Ni(Ⅱ)化合物表现出典型的变磁行为,其反铁磁有序的临界温度为T_N=6.5K,场诱导铁磁相变的临界磁场为Hc=1.35KOe。有趣的是,上述化合物中层间堆积导致一种含一维开放通道的结构,通道内含配位和非配位的水分子。XRD表征分析表明它们在失去溶剂水和配位水分子后可以得到一种新的物相,而该物相在水气氛中放置一段时间又可以回复为原有结构。基于这种可逆的物相变化,我们研究了溶剂对Co(Ⅱ)、Ni(Ⅱ)化合物磁性的影响。其中最值得一提的是Ni化合物呈现溶剂调控的磁性,在脱/吸水前后变磁行为有明显变化,脱水后材料的临界温度和变磁临界场均大幅度升高(T_N=13.2K,H_C=23.5KOe),并表现出特殊的磁滞行为,这些现象可归因于脱水后链间反铁磁相互作用的增强。这类溶剂调制的变磁材料有可能在磁性传感等领域获得应用。
3吡啶羧酸类配体同过渡金属的化合物:同时含有可参与配位的N原子和羧酸O原子的吡啶羧酸类配体因其不对称桥联特性而受到广泛关注。我们将3-或4-吡啶丙烯酸(3-Hpya,4-Hpya)引入到类卤素桥配合物体系,设计合成了一系列叠氮或硫氰酸根桥联的Cd(Ⅱ)、Cu(Ⅱ)配位聚合物。(1)对Cd(Ⅱ)-硫氰酸根体系,我们主要分析讨论了溶剂等反应条件、有机配体取代位置及去质子化程度对产物配位结构和氢键作用的影响。其中使用高氯酸盐得到的化合物中,配体3-pya和4-pya质子化(3-pya的羧酸基团质子化而4-pyag比啶环上的氮原子质子化)只能通过其一端的吡啶氮原子或羧酸基团配位从而得到一维链结构;当使用醋酸盐时,则上述两个配体完全脱质子,其吡啶氮原子和羧基氧原子同时参与配位,得到两维结构。究其原因,可能是使用不同的金属Cd(Ⅱ)盐,会对整个反应体系的酸碱度产生一定的影响。(2) 4-pya配体和金属Cu(Ⅱ)-叠氮共同得到的化合物是基于双EO叠氮桥联双核单元的二维配位聚合物。这种含有两重EO叠氮桥联的双核Cu(Ⅱ)化合物是用于分析解释磁构关系的一种十分简单实用的模型。
Great efforts have been expended on the organic ligands containing carboxylate groups because of their fascinating structural diversity;this kind of ligands can offer great potentials for fine control over coordination architectures and applications in catalysis,luminescence,magnetism and porosity.Meanwhile,the study on the azido and thiocyanate ions has attracted more and more attention due to their significant contribution to magnetic coupling.Recently,a large number of compounds contain azido-carboxylate mixed bridges have been obtained.These two kinds of bridges have different influence on the magnetic properties.With this aims,dicarboxylates are used as bridging ligands between divalent transition metal ions,in combination with the use of azido or thiocyanate ions bridging ligands,twenty-four new coordination polymers,including one dimensional,two dimensional and three dimensional motifs, have been prepared,and the magnetic properties of some of the complexes have been characterized.
1.Solvothermal reactions of dimethyl pyridazine-3,6-dicarboxylate and appropriate metal chlorides in the absence/presence of KCl,NaCl or NH_4Cl yielded a series of coordination compounds of pyridazine-3,6-dicarboxylate with Mn(Ⅱ),Co(Ⅱ),Ni(Ⅱ) and Zn(Ⅱ).All the Mn(Ⅱ) compounds contain the anionic binuclear motif [Mn_2(pzdc)_3]~(2-) with the trigonal prismatic shape.Through the K/Na-O electrostatic coordination,charge-assisted N-H/O hydrogen bonds,and weak C-H/O hydrogen-bonds,the binuclear prismatic anion co-assembles with different cations ([Mn(H_2O)_6]~(2+),K~+,Na~+ or NH_4~+) to generate 3D architectures.Under similar synthetic conditions,the Co(Ⅱ) and Ni(Ⅱ) ions always give the neutral binuclear molecules[M_2(pzdc)_2(H_2O)_4],which are self-assembled into 3D hydrogen-bonded networks.The Zn(Ⅱ) ion seems to be amphibious:in the presence of NH_4~+,K~+ and Na~+,it forms the[Zn_2(pzdc)_3]~(2-) species that are isostructural with the Mn(Ⅱ) species, but the absence of the above cations leads to[Zn_2(pzdc)_2(H_2O)_4],which is isomorphous with the Co(Ⅱ) and Ni(Ⅱ) compounds.The different structures have been qualitatively explained based on the metal ionic size,ligand constraints, inter-ligand repulsion,ligand-field effects,and anionic-cationic interactions. Magnetic studies on selected Mn(Ⅱ) compounds reveal that weak antiferromagnetic coupling is operative through the triple pyridazine bridges within the prismatic anions. 2.A novel 2D coordination polymer consisting of ferromagnetic Ni(Ⅱ) chains with alternating double EO-azide bridges and(EO-azide)bis(carboxylate) triple bridges exhibits Solvent-modulated metamagnetism,and the reversible dehydration/hydration processes are accompanied by significant changes in critical temperature,critical field and hysteresis.Then another two compounds of Co(Ⅱ) and Mn(Ⅱ) that have the similar structure with the Ni(Ⅱ) compound were synthesized,and their reversible dehydration/hydration processes and the magnetic properties were analysed.By comparison,the(EO-azide)bis(carboxylate) triple bridges in Ni(Ⅱ) or Co(Ⅱ) chains mediate ferromagnetic interaction while this kind of bridge in Mn(Ⅱ) chain mediates antiferromagnetic interaction.
3.Four new cadmium(Ⅱ) coordination polymers have been synthesized from appropriate Cd(Ⅱ) salts and 4-pyridylacrylic acid(4-Hpya) or 3-pyridylacrylic acid (3-Hpya) in the presence of thiocyanate under similar hydrothermal conditions.The use of cadmium perchlorate as metal source leads to complexes with 4-Hpya and 3-Hpya,while the use of cadmium acetate leads to complexes with 4-pya~- and 3-pya~-. Whether the ligand is protonated or not has much influence on the structure of these cmpounds,and the proton can plays an important role in assembling the chains into higher-dimensional networks via hydrogen-bonds.Besides,a Cu(Ⅱ) complex with azide and 4-Hpya has been synthesized and characterized crystallographically and spectroscopically,and the magneto-structural correlations have been discussed in comparison with other Cu(Ⅱ) dimers with the same bridging motif.
1哒嗪二甲酸的配位化学及抗衡离子对晶体结构组装的影响:(1)首先,我们采用3,6-哒嗪二甲酸(H_2pzdc)配体与金属Mn(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)及Zn(Ⅱ)离子在水热条件下合成得到了一系列双核化合物。其中最值得一提的是Mn(Ⅱ)形成的结构独特的双核阴离子[Mn_2(pzdc)_3]~(2-),该化合物中三个pzdc配体围绕一个C_3对称轴与两个金属离子配位,形成三棱柱结构。而金属Co(Ⅱ)、Ni(Ⅱ)或Zn(Ⅱ)形成一种边边配位的中性平面分子[M_2(pzdc)_2(H_2O)_4]。这种结构差异的出现可以归因于这些金属离子半径的差异。(2)在Mn(Ⅱ)的化合物中,三棱柱阴离子[Mn_2(pzdc)_3]~(2-)单元有丰富的未配位羧酸氧原子,以这些氧原子为潜在的配位点或是氢键受体,可以将这种阴离子结构当做“配合物配体”用于构建新的金属-有机配位聚合网络或氢键超分子网络。考虑到这种配合物配体策略,我们在合成化合物的过程中引入了抗衡离子(NH_4~+,K~+或Na~+)从而得到了一系列金属Mn(Ⅱ)和Zn(Ⅱ)的化合物。这些化合物都包含双核三棱柱结构单元[M_2(pzdc)_3]~(2-),这种阴离子单元又可以和不同的阳离子(NH_4~+,K~+或Na~+)连接形成三维的配位或氢键网络。然而对于金属Co(Ⅱ)和Ni(Ⅱ)的体系中,不管是否引入抗衡离子,都只能得到上述的边边配位的中性分子结构。
2含甜菜碱类共配体的叠氮-羧基混桥化合物的结构与磁性:叠氮离子在与负电性羧酸根离子的配位竞争中处于劣势,因此利用通常的二羧酸配体难以得到叠氮-羧基混桥配合物。我们试图通过降低二羧酸配体的负电荷来降低二羧酸配体的竞争能力,使之与叠氮配体相匹配,从而得到含有羧酸-叠氮混桥的化合物。基于这种策略,我们采用了甜菜碱类双羧酸有机配体,以这种配体作为辅助配体,在叠氮存在下,与金属Ni(Ⅱ),Co(Ⅱ),Mn(Ⅱ)和Cu(Ⅱ)配位得到了一系列叠氮-羧基混桥化合物,其中Ni、Co、Mn的化合物是同晶结构。其中金属离子通过叠氮-羧基三重桥(一个EO叠氮桥和两个syn-syn羧基桥)和两重EO叠氮桥连接成负电性聚合链,链间又通过正电性有机基团连接成层。磁性研究表明上述三重桥在Co(Ⅱ)、Ni(Ⅱ)化合物中传递铁磁交换,而在Mn(Ⅱ)化合物中传递反铁磁交换。Ni(Ⅱ)化合物表现出典型的变磁行为,其反铁磁有序的临界温度为T_N=6.5K,场诱导铁磁相变的临界磁场为Hc=1.35KOe。有趣的是,上述化合物中层间堆积导致一种含一维开放通道的结构,通道内含配位和非配位的水分子。XRD表征分析表明它们在失去溶剂水和配位水分子后可以得到一种新的物相,而该物相在水气氛中放置一段时间又可以回复为原有结构。基于这种可逆的物相变化,我们研究了溶剂对Co(Ⅱ)、Ni(Ⅱ)化合物磁性的影响。其中最值得一提的是Ni化合物呈现溶剂调控的磁性,在脱/吸水前后变磁行为有明显变化,脱水后材料的临界温度和变磁临界场均大幅度升高(T_N=13.2K,H_C=23.5KOe),并表现出特殊的磁滞行为,这些现象可归因于脱水后链间反铁磁相互作用的增强。这类溶剂调制的变磁材料有可能在磁性传感等领域获得应用。
3吡啶羧酸类配体同过渡金属的化合物:同时含有可参与配位的N原子和羧酸O原子的吡啶羧酸类配体因其不对称桥联特性而受到广泛关注。我们将3-或4-吡啶丙烯酸(3-Hpya,4-Hpya)引入到类卤素桥配合物体系,设计合成了一系列叠氮或硫氰酸根桥联的Cd(Ⅱ)、Cu(Ⅱ)配位聚合物。(1)对Cd(Ⅱ)-硫氰酸根体系,我们主要分析讨论了溶剂等反应条件、有机配体取代位置及去质子化程度对产物配位结构和氢键作用的影响。其中使用高氯酸盐得到的化合物中,配体3-pya和4-pya质子化(3-pya的羧酸基团质子化而4-pyag比啶环上的氮原子质子化)只能通过其一端的吡啶氮原子或羧酸基团配位从而得到一维链结构;当使用醋酸盐时,则上述两个配体完全脱质子,其吡啶氮原子和羧基氧原子同时参与配位,得到两维结构。究其原因,可能是使用不同的金属Cd(Ⅱ)盐,会对整个反应体系的酸碱度产生一定的影响。(2) 4-pya配体和金属Cu(Ⅱ)-叠氮共同得到的化合物是基于双EO叠氮桥联双核单元的二维配位聚合物。这种含有两重EO叠氮桥联的双核Cu(Ⅱ)化合物是用于分析解释磁构关系的一种十分简单实用的模型。
Great efforts have been expended on the organic ligands containing carboxylate groups because of their fascinating structural diversity;this kind of ligands can offer great potentials for fine control over coordination architectures and applications in catalysis,luminescence,magnetism and porosity.Meanwhile,the study on the azido and thiocyanate ions has attracted more and more attention due to their significant contribution to magnetic coupling.Recently,a large number of compounds contain azido-carboxylate mixed bridges have been obtained.These two kinds of bridges have different influence on the magnetic properties.With this aims,dicarboxylates are used as bridging ligands between divalent transition metal ions,in combination with the use of azido or thiocyanate ions bridging ligands,twenty-four new coordination polymers,including one dimensional,two dimensional and three dimensional motifs, have been prepared,and the magnetic properties of some of the complexes have been characterized.
1.Solvothermal reactions of dimethyl pyridazine-3,6-dicarboxylate and appropriate metal chlorides in the absence/presence of KCl,NaCl or NH_4Cl yielded a series of coordination compounds of pyridazine-3,6-dicarboxylate with Mn(Ⅱ),Co(Ⅱ),Ni(Ⅱ) and Zn(Ⅱ).All the Mn(Ⅱ) compounds contain the anionic binuclear motif [Mn_2(pzdc)_3]~(2-) with the trigonal prismatic shape.Through the K/Na-O electrostatic coordination,charge-assisted N-H/O hydrogen bonds,and weak C-H/O hydrogen-bonds,the binuclear prismatic anion co-assembles with different cations ([Mn(H_2O)_6]~(2+),K~+,Na~+ or NH_4~+) to generate 3D architectures.Under similar synthetic conditions,the Co(Ⅱ) and Ni(Ⅱ) ions always give the neutral binuclear molecules[M_2(pzdc)_2(H_2O)_4],which are self-assembled into 3D hydrogen-bonded networks.The Zn(Ⅱ) ion seems to be amphibious:in the presence of NH_4~+,K~+ and Na~+,it forms the[Zn_2(pzdc)_3]~(2-) species that are isostructural with the Mn(Ⅱ) species, but the absence of the above cations leads to[Zn_2(pzdc)_2(H_2O)_4],which is isomorphous with the Co(Ⅱ) and Ni(Ⅱ) compounds.The different structures have been qualitatively explained based on the metal ionic size,ligand constraints, inter-ligand repulsion,ligand-field effects,and anionic-cationic interactions. Magnetic studies on selected Mn(Ⅱ) compounds reveal that weak antiferromagnetic coupling is operative through the triple pyridazine bridges within the prismatic anions. 2.A novel 2D coordination polymer consisting of ferromagnetic Ni(Ⅱ) chains with alternating double EO-azide bridges and(EO-azide)bis(carboxylate) triple bridges exhibits Solvent-modulated metamagnetism,and the reversible dehydration/hydration processes are accompanied by significant changes in critical temperature,critical field and hysteresis.Then another two compounds of Co(Ⅱ) and Mn(Ⅱ) that have the similar structure with the Ni(Ⅱ) compound were synthesized,and their reversible dehydration/hydration processes and the magnetic properties were analysed.By comparison,the(EO-azide)bis(carboxylate) triple bridges in Ni(Ⅱ) or Co(Ⅱ) chains mediate ferromagnetic interaction while this kind of bridge in Mn(Ⅱ) chain mediates antiferromagnetic interaction.
3.Four new cadmium(Ⅱ) coordination polymers have been synthesized from appropriate Cd(Ⅱ) salts and 4-pyridylacrylic acid(4-Hpya) or 3-pyridylacrylic acid (3-Hpya) in the presence of thiocyanate under similar hydrothermal conditions.The use of cadmium perchlorate as metal source leads to complexes with 4-Hpya and 3-Hpya,while the use of cadmium acetate leads to complexes with 4-pya~- and 3-pya~-. Whether the ligand is protonated or not has much influence on the structure of these cmpounds,and the proton can plays an important role in assembling the chains into higher-dimensional networks via hydrogen-bonds.Besides,a Cu(Ⅱ) complex with azide and 4-Hpya has been synthesized and characterized crystallographically and spectroscopically,and the magneto-structural correlations have been discussed in comparison with other Cu(Ⅱ) dimers with the same bridging motif.
引文
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